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Arsine Detection using Chemcassette® Technology
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History
• In 1998 ACGIH proposed changing the TLV for AsH3 from 50 ppb to 2 ppb
• In 2007 ACGIH changed the TLV for AsH3 from 50 ppb to 5 ppb
• Honeywell Analytics has already developed a higher sensitivity and longer lasting Chemcassette®
• Study data supported the ability for HA to meet the proposed lower TLV level for AsH3
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Development
• The increased sensitivity of the new formulation allowed Honeywell Analytics to achieve better lower detectable limits for all equipment, as shown
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Gas Monitors’ Low Detection Limit Improvement
AsH3 PH3 SiH4 B2H6
Monitor XP TapeStandard
TapeXP Tape
StandardTape
XP TapeStandard
TapeXP Tape
StandardTape
Vertex/CM4 0.3 ppb 5 ppb 5 ppb 5 ppb 0.25 ppb 0.5 ppb 10 ppb 15 ppb
System 16 0.7 ppb 7 ppb 8 ppb 10 ppb 0.4 ppb 1.33 ppb 13 ppb 21 ppb
SPM 0.7 ppb 15 ppb 20 ppb 30 ppb 0.25 ppb 0.5 ppb 10 ppb 30 ppb
TLD 0.7 ppb 15 ppb 20 ppb 30 ppb 0.25 ppb 0.5 ppb 10 ppb 30 ppb
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Sensitivity Aging Results
• Honeywell Analytics also tested for Chemcassette® sensitivity. Would the formula remain consistent over three months?
Day 1 Day 14 Day 42 Day 77 Day 122
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Gas Generation Methodology• Apparatus A: gas source with 2 certified AsH3 gas cylinders
• Apparatus B: Kin-Tech gas generation with permeation device
• Concentrations determined by theoretical calculations, and confirmed by 3 standard methods
First Stage Gas
Mixing Chamber
Dilution AirConcentrated AsH3
AsH3 Gas(from cylinder orpermeation tube
standard gasgenerator)
FilteredCompressed
Air
Samplerfor quantitative
analysis
Mass Flow Controller0-500 ml/min
Vertex Gas Monitor
CM4Gas Monitor
SPMGas Monitor
System16 Gas Monitor
Mass Flow Controller1-20 l/min
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Validation Methods
• Honeywell verified standard gas concentrations using 3 independent methods
– FTIR (64 scans with a 10 m cell)– Analytical method (Visible spectrophotometry based on NIOSH method S332)– Kin-Tech Standard Gas Generator (Permeation Device Method)
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Gas Cylinder Consistency Test
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Signal to Noise Ratio
• To validate instrument response, Honeywell Analytics did extensive “noise level” studies both in the laboratory and in the field
• A new LDL (lower detection limit) was determined by finding an acceptable signal to noise ratio
• Ratio was set at >3:1 signal to noise
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CM4® Low Concentration AsH3 Signal and Noise
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System16 Low Concentration AsH3 Signal and Noise
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SPM Low Concentration AsH3 Signal and Noise
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Ambient RH vs. Noise Test
• Normal RH setting in semiconductor fabs is about 40%• Extensive studies were done on noise levels at 5% RH, at
40% RH and at 90% RH versus the signal generated by 0.5 ppb AsH3 (one tenth of the proposed TLV level)
• Maximum noise drift caused by shifting RH from 5 to 40% is 10 cts.
• This is less than 1/10th the signal generated by 0.5 ppb of AsH3
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CM4® Ambient RH Noise vs. 0.5 ppb AsH3 Signal
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CM4® Low Level Calibration Accuracy Verification II
Test 1 Test 2 Test 3 Test 4 Test 5 Test 6 Test 7 Test 8
Oven Temperature (°C) 30 30 30 50 50 50 60 60
Room RH (%) 50 48 48 51 50 52 50 49
Gas RH (%) 40 40 40 40 40 40 40 40
Total Output Flow* (ml/min) 3273 3273 3273 3273 3273 3273 3273 3273
Cylinder Pressure (psi) 50 50 50 55 55 55 55 55
Permeation Oven Temperature (°C) 30 30 30 50 50 50 60 60
Permeation Rate (nl/min) 140.84 140.84 140.84 283.39 283.39 283.39 390.36 390.36
KT Gas Concentration (ppb) 43.03 43.03 43.03 86.58 86.58 86.58 119.27 119.27
KT-Gas Flow (ml/min) 230 110 80 245 560 950 3273 3273
Dilution Air Flow (L/min) 10.05 10.05 10.05 10.07 10.07 7.6 16.2 4.5
Standard Gas Concentration (ppb) 0.96 0.47 0.34 2.06 4.56 9.62 20.05 50.22
CM4 Response (ppb) 0.98 0.5 0.32 2.3 5.2 10.1 21.5 52
CM4 Response/Standard Gas (ppb) 102.08% 107.32% 94.16% 11.84% 114.00% 104.98% 107.25% 103.55%
Standard Gas Source: Standard Gas Generator with Permeation Device
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CM4® Low Level Calibration Accuracy Verification IIStandard Gas Source: Standard Gas Generator with Permeation Device
Std Gas Conc (ppb)
CM4 (ppb) Accuracy
0.96 0.98 102.08%
0.47 0.5 107.32%
0.34 0.32 94.16%
2.06 2.3 111.84%
4.56 5.2 114.00%
9.62 10.1 104.98%
20.05 21.5 107.25%
50.22 52 103.55%
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CM4® XP Result Consistency Over Time
• Before placing an XP CM4® at a Beta site, the CM4® was tested for consistency over time in laboratory condition
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Beta Testing Data
• Beta Customer ran sample lines from the test CM4® to existing monitoring locations at the tool, also in the fab utility area, and to VMBs located in the sub-fab
• The CM4® was run “in situ” for over three months• Data was collected by the Customer and transmitted to
Honeywell Analytics
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CM4® AsH3 Low Detection Limit Feasibility Field Study
Beta Testing Site A, Test Result I
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CM4® AsH3 Low Detection Limit Feasibility Field Study
Beta Testing Site A, Test Result II
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CM4® AsH3 Low Detection Limit Feasibility Field Study
Beta Testing Site A, Test Result III
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CM4® AsH3 Low Detection Limit Feasibility Field Study
Beta Testing Site A, Test Result IV
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CM4® AsH3 Low Detection Limit Feasibility Field Study
Beta Testing Site A, Test Result V
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Conclusion
• Based on Lab work, proof of methodology, and field trials, Chemcassette Technology can successfully monitor for AsH3 at the newly established level of 5 ppb without risk of false positives.
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Questions??